The suggested method depends upon the determination of lobeline, khellin and emetine hydrochloride. The method is simple, accurate, precise, and depends on the quantitative TLC spectrodensitometric evaluation of lobeline I, khellin II, and emetine hydrochloride III. Excellent separation with discrete spots was quickly obtained. The proposed method determines 8.50−22.00 mg.mL−1, 0.02−0.14 mg.mL−1, and 0.8−3.6 mg.mL−1with mean percentage accuracies of 99.34% ± 0.49%, 99.99% ± 0.62%, and 99.69% ± 0.50% for I, II, and III respectively.